US4632686A - Method of manufacturing quartz glass crucibles with low bubble content - Google Patents

Method of manufacturing quartz glass crucibles with low bubble content Download PDF

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Publication number
US4632686A
US4632686A US06/832,614 US83261486A US4632686A US 4632686 A US4632686 A US 4632686A US 83261486 A US83261486 A US 83261486A US 4632686 A US4632686 A US 4632686A
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quartz
mold
vacuum
crucible
tooling
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US06/832,614
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David R. Brown
Charles E. Frost, Jr.
Kenneth A. White
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Osram Sylvania Inc
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GTE Products Corp
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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
    • C03B19/095—Other methods of shaping glass by fusing powdered glass in a shaping mould by centrifuging, e.g. arc discharge in rotating mould

Definitions

  • This invention relates to an improved method for manufacturing quartz glass crucibles of low bubble content for use in making monocrystalline silicon for semiconductor applications.
  • quartz crucibles It is general practice to make quartz crucibles by pouring crystalline quartz sand or amorphous quartz powder into the interior of a mold which rotates around a vertical axis. The rotation holds the starting material against the mold walls by centrifugal force. Heat is then generated by an electric arc, or other means, to the interior of the mold to fuse the particles into an amorphous glass. Fusion will start at the interior surface and gradually melt glass toward the relatively cooler mold. The process will continue until an adequate thickness of glass is formed and a layer of calcined material will be left between the quartz crucible and mold. The crucible can then be removed from the mold.
  • U.S. Pat. No. 4,416,680 discloses a method in which crystalline quartz sand or amorphous quartz powder is introduced into a rotating mold which has small holes approximately 0.5 mm diameter for applying a vacuum on the quartz material.
  • a vacuum pump is used to obtain a pressure less than 5000 Pa, and preferably less than 1000 Pa, in a vacuum cavity travelling to the mold.
  • the vacuum is applied to the outside of the quartz material. When the material is heated and melted, the vacuum applied will remove gas from the material as it is melted, resulting in a quartz glass low in bubble content.
  • the problem with using the mold with 0.5 mm holes for the vacuum is that bridging of the quartz particles is not always certain and some particles will go through the holes.
  • the 0.5 mm diameter holes offer high resistance to the vacuum. Since the vacuum actually reaching the quartz is not great, this process will not be optimum for removing all bubbles.
  • Another disadvantage to this method is that the mold cost is very high due to considerable machining costs of drilling many 0.5 mm diameter holes, especially if made in a hard material such as the steel referenced in that patent.
  • This invention discloses a method for making quartz crucibles of lower bubble content than prior art methods.
  • the first material used that is, the material in contact with the mold, is relatively coarse quartz material. This permits ready transfer of vacuum therethrough.
  • the second material used that is, the material overlying the first material, is relatively fine quartz material. This second material packs denser than the first material with the result that less air will pass therethrough, thereby improving the vacuum that is removing the gas bubbles.
  • the first material used will have a particle size distribution all between about 297 microns and 105 microns.
  • the material will pack so that gas will pass through it.
  • a layer of finely ground crystalline quartz or amorphous quartz is introduced around the entire inside surface.
  • This comminuted material is considerably smaller than that used in prior art methods. Its particles will all range in size between about 120 microns and 44 microns.
  • This fine material will pack more densely and become a block to the ambient air being drawn in at the inside surface. This results in less loss of vacuum due to ambient air coming in from the inside of the mold.
  • a higher vacuum is obtained on the quartz starting material which is indicated by an increase in vacuum at a vacuum gauge on the vacuum line connected to the tooling. The higher vacuum will be capable of removing gas either trapped as voids or gas generated by heating the quartz material when the heat source is introduced to the material.
  • the absence of bubbles within the wall of the quartz glass and especially near the inside surface, is extremely important to the silicon crystal growers.
  • the absence of bubbles inside the glass and close to the interior surface is desirable because the inside surface of the quartz crucibles is dissolved away for approximately 1 mm during the crystal growing process. Any bubbles in this area can possibly be uncovered or rupture and introduce a quartz particulate into the silicon melt.
  • vacuum type crystal pullers the gas pressure inside the bubble is a critical factor. If the pressure inside the bubble is higher than that of the vacuum inside the furnace, and at temperatures which the crucible is heated, the pressure inside the bubble can increase and the viscosity of the quartz at these temperatures is low enough so that bubbles will expand in size. This expansion can cause the bubble near the inside surface to rupture into the melt, releasing quartz particulates.
  • a quartz particulate can interrupt the single crystal process or end up in the silicon crystal.
  • Bubbles which get uncovered during the crystal growing process can also be the site for the formation of cooled silicon which will solidify and start the formation of a secondary crystal from the quartz crucible. This secondary crystal can grow into the melt and interrupt the crystal growing process.
  • the lack of bubbles within the glass can also increase the strength of the quartz crucible structure at high temperatures since the viscosity of the quartz decreases at these temperatures to the point where the crucible can sag or sump.
  • the absence of voids will leave more material to hold up the weight of the glass above it.
  • the drawing illustrates apparatus useful for repetitive manufacture of quartz crucibles having low bubble content.
  • An exterior housing 1 has separate cavities (not shown) for water cooling and for applying a vacuum to the tooling mold 2.
  • Water cooled molds are preferred to uncooled molds to maintain life and dimensional stability of the molds, which can oxidize at extreme temperatures needed to melt the quartz.
  • the entire housing and mold assembly is rotated using an external drive motor 6 and a rotating spindle 7.
  • the rotating spindle assembly 7 is capable of transferring vacuum to the housing 1.
  • the spindle 7 also has another fitting 8 within to transfer water to and from the housing 1.
  • the spindle 7 and housing 1 rotate as indicated by arrow 9. Vacuum is applied to the housing 1 and spindle 7 through a pipe 10.
  • Suitable vacuum can be supplied by a pump 13 rated at least at 40 cfm, preferably 100 cfm.
  • a vacuum gage 11 is used for monitoring pressure corresponding to pressure in the vacuum cavities.
  • First quartz material 3 is poured into mold 2 and then finer second quartz material 4 is poured thereover, to cover material 3.
  • Material 4 immediately increases the vacuum by about 75 to 100 mm Hg, as read on gauge 11.
  • Mold tooling 2 can be either graphite or heat resistant steel alloy.
  • Quartz materials 3 and 4 inside the mold are then heated with an electric arc produced between electrodes 17 which will first sinter and then melt the material.
  • the interior surface of material 3 will start to melt first which seals the vacuum even further from the inside of cavity 16 at ambient conditions. The vacuum at this point will increase further.
  • the fine quartz material, packed densely, will fuse into glass low in microscopic bubble content. The heat will fuse the glass thicker and the process will be stopped when a suitable thickness is formed.
  • the entire cross section of the glass will be substantially free of bubbles; only a few microscopic bubbles will remain.
  • the addition of finer quartz to the inside surface significantly reduces bubbles including microscopic bubbles to a level lower than that obtained in the prior art.
  • the vacuum and rotation are maintained throughout the heating process to remove bubbles and maintain dimensions of the crucible.
  • the crucible can be removed from the tooling 2 by closing valve 14 to the vacuum pump and opening valve 19 to the compressed air source 15, which will pressurize the vacuum cavity and force the crucible out.
  • the tooling 2 can also be made in two pieces, a removable sleeve and a non-removable base, for removing the crucible.
  • the crucible will stay inside the sleeve when it is removed and then the remaining sand between the tooling and the crucible can be tapped or vibrated out to free the crucible.
  • This process is also enchanced by using water cooled tooling because during fusion of the glass, high temperatures are generated which oxidize and erode the tooling.
  • the layer of quartz sand remaining between the crucible and tooling will not stop the slow oxidation of the tooling over time, whether the tooling is graphite or a heat resistant steel, without water cooling. Therefore, having water cooled tooling is an advantage for tooling life and to lower the cost of manufacturing.
  • the heat generated in the process will also expand the tooling during the fusion process to the point that when the process is complete, the tooling will contract and make it difficult or impossible to remove the crucible.
  • the thermal expansion of quartz is much less than that of the tooling so that the tooling will compress the crucible and even crack it. This compression is minimized by using water cooled tooling kept at a constant water temperature during the process. This will reduce expansion and contraction of the tooling so that the crucible will be easy to remove.
  • the expansion, contraction and oxidation of the tooling could also be reduced by designing the tooling with a larger inside diameter to leave more quartz starting material to be left over between the crucible and the tooling.
  • the thicker amount of sand will insulate the tooling from the heat so that it will not oxidize as rapidly or expand and contract as much to facilitate in crucible removal.
  • This process is costly because significantly more of the expensive starting material is used.
  • the cost of the high purity starting material is so high that it is impractical to waste it by using any excess during the process.
  • the starting material left over after fusion is not suitable for reuse in the semiconductor grade crucible process since it will contain impurities from the tooling. Therefore it is wise to use only a minimal amount of insulative sand for a barrier to react with the tooling and for heat insulation.
  • Finely ground quartz material 4 can be obtained through a variety of means, but preferably in a mill using quartz glass pieces as the media.
  • the mill container should also be made of a cylindrical polypropylene material or a cylindrical quartz tube with quartz end plates.
  • the quartz glass media used to grind the material were approximately 6 cm square and 7.5 mm thick. Either crystalline quartz sand or amorphous quartz glass can be ground into fine material.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

In the manufacture of a quartz glass crucible of low bubble content, a first layer of granular quartz material is disposed on the interior of a rotating mold through the walls of which a vacuum can be drawn. A second layer of finer quartz material is then disposed on the first layer. The quartz material is then heated, melted and fused to form a crucible.

Description

This invention relates to an improved method for manufacturing quartz glass crucibles of low bubble content for use in making monocrystalline silicon for semiconductor applications.
It is general practice to make quartz crucibles by pouring crystalline quartz sand or amorphous quartz powder into the interior of a mold which rotates around a vertical axis. The rotation holds the starting material against the mold walls by centrifugal force. Heat is then generated by an electric arc, or other means, to the interior of the mold to fuse the particles into an amorphous glass. Fusion will start at the interior surface and gradually melt glass toward the relatively cooler mold. The process will continue until an adequate thickness of glass is formed and a layer of calcined material will be left between the quartz crucible and mold. The crucible can then be removed from the mold.
U.S. Pat. No. 4,416,680 discloses a method in which crystalline quartz sand or amorphous quartz powder is introduced into a rotating mold which has small holes approximately 0.5 mm diameter for applying a vacuum on the quartz material. A vacuum pump is used to obtain a pressure less than 5000 Pa, and preferably less than 1000 Pa, in a vacuum cavity travelling to the mold. The vacuum is applied to the outside of the quartz material. When the material is heated and melted, the vacuum applied will remove gas from the material as it is melted, resulting in a quartz glass low in bubble content. The problem with using the mold with 0.5 mm holes for the vacuum is that bridging of the quartz particles is not always certain and some particles will go through the holes. Also, the 0.5 mm diameter holes offer high resistance to the vacuum. Since the vacuum actually reaching the quartz is not great, this process will not be optimum for removing all bubbles. Another disadvantage to this method is that the mold cost is very high due to considerable machining costs of drilling many 0.5 mm diameter holes, especially if made in a hard material such as the steel referenced in that patent.
Another method described in the patent involves the use of a porous material as the mold capable of transferring vacuum. The disadvantage to using this material is that it will oxidize rapidly, react with the quartz material and have extremely short life, especially if not cooled during the process. The initial cost of this type of mold is high and would not be economical for a repetitive manufacturing process.
This invention discloses a method for making quartz crucibles of lower bubble content than prior art methods.
In this invention two sizes of granular quartz material are used. The first material used, that is, the material in contact with the mold, is relatively coarse quartz material. This permits ready transfer of vacuum therethrough. The second material used, that is, the material overlying the first material, is relatively fine quartz material. This second material packs denser than the first material with the result that less air will pass therethrough, thereby improving the vacuum that is removing the gas bubbles.
The first material used will have a particle size distribution all between about 297 microns and 105 microns. The material will pack so that gas will pass through it. On the inside of this material, a layer of finely ground crystalline quartz or amorphous quartz is introduced around the entire inside surface. This comminuted material is considerably smaller than that used in prior art methods. Its particles will all range in size between about 120 microns and 44 microns. This fine material will pack more densely and become a block to the ambient air being drawn in at the inside surface. This results in less loss of vacuum due to ambient air coming in from the inside of the mold. A higher vacuum is obtained on the quartz starting material which is indicated by an increase in vacuum at a vacuum gauge on the vacuum line connected to the tooling. The higher vacuum will be capable of removing gas either trapped as voids or gas generated by heating the quartz material when the heat source is introduced to the material.
When the fine material, which is the first to fuse, becomes glass, it will fuse to a glass with extremely low bubble content near the surface due to its dense packing and high vacuum. When the inside surface becomes glass, it seals over the raw material and the vacuum will increase even further, for the remainder of the heating process.
The absence of bubbles within the wall of the quartz glass and especially near the inside surface, is extremely important to the silicon crystal growers. The absence of bubbles inside the glass and close to the interior surface is desirable because the inside surface of the quartz crucibles is dissolved away for approximately 1 mm during the crystal growing process. Any bubbles in this area can possibly be uncovered or rupture and introduce a quartz particulate into the silicon melt. In vacuum type crystal pullers the gas pressure inside the bubble is a critical factor. If the pressure inside the bubble is higher than that of the vacuum inside the furnace, and at temperatures which the crucible is heated, the pressure inside the bubble can increase and the viscosity of the quartz at these temperatures is low enough so that bubbles will expand in size. This expansion can cause the bubble near the inside surface to rupture into the melt, releasing quartz particulates. A quartz particulate can interrupt the single crystal process or end up in the silicon crystal.
Bubbles which get uncovered during the crystal growing process can also be the site for the formation of cooled silicon which will solidify and start the formation of a secondary crystal from the quartz crucible. This secondary crystal can grow into the melt and interrupt the crystal growing process.
The lack of bubbles within the glass can also increase the strength of the quartz crucible structure at high temperatures since the viscosity of the quartz decreases at these temperatures to the point where the crucible can sag or sump. The absence of voids will leave more material to hold up the weight of the glass above it.
The drawing illustrates apparatus useful for repetitive manufacture of quartz crucibles having low bubble content.
An exterior housing 1 has separate cavities (not shown) for water cooling and for applying a vacuum to the tooling mold 2. Water cooled molds are preferred to uncooled molds to maintain life and dimensional stability of the molds, which can oxidize at extreme temperatures needed to melt the quartz. The entire housing and mold assembly is rotated using an external drive motor 6 and a rotating spindle 7. The rotating spindle assembly 7 is capable of transferring vacuum to the housing 1. The spindle 7 also has another fitting 8 within to transfer water to and from the housing 1. The spindle 7 and housing 1 rotate as indicated by arrow 9. Vacuum is applied to the housing 1 and spindle 7 through a pipe 10. Suitable vacuum can be supplied by a pump 13 rated at least at 40 cfm, preferably 100 cfm. A vacuum gage 11 is used for monitoring pressure corresponding to pressure in the vacuum cavities.
First quartz material 3 is poured into mold 2 and then finer second quartz material 4 is poured thereover, to cover material 3. Material 4 immediately increases the vacuum by about 75 to 100 mm Hg, as read on gauge 11. Mold tooling 2 can be either graphite or heat resistant steel alloy.
Quartz materials 3 and 4 inside the mold are then heated with an electric arc produced between electrodes 17 which will first sinter and then melt the material. The interior surface of material 3 will start to melt first which seals the vacuum even further from the inside of cavity 16 at ambient conditions. The vacuum at this point will increase further. The fine quartz material, packed densely, will fuse into glass low in microscopic bubble content. The heat will fuse the glass thicker and the process will be stopped when a suitable thickness is formed. The entire cross section of the glass will be substantially free of bubbles; only a few microscopic bubbles will remain. The addition of finer quartz to the inside surface significantly reduces bubbles including microscopic bubbles to a level lower than that obtained in the prior art. The vacuum and rotation are maintained throughout the heating process to remove bubbles and maintain dimensions of the crucible.
When the heating process is complete, the crucible can be removed from the tooling 2 by closing valve 14 to the vacuum pump and opening valve 19 to the compressed air source 15, which will pressurize the vacuum cavity and force the crucible out. The tooling 2 can also be made in two pieces, a removable sleeve and a non-removable base, for removing the crucible.
The crucible will stay inside the sleeve when it is removed and then the remaining sand between the tooling and the crucible can be tapped or vibrated out to free the crucible.
This process is also enchanced by using water cooled tooling because during fusion of the glass, high temperatures are generated which oxidize and erode the tooling. The layer of quartz sand remaining between the crucible and tooling will not stop the slow oxidation of the tooling over time, whether the tooling is graphite or a heat resistant steel, without water cooling. Therefore, having water cooled tooling is an advantage for tooling life and to lower the cost of manufacturing.
The heat generated in the process will also expand the tooling during the fusion process to the point that when the process is complete, the tooling will contract and make it difficult or impossible to remove the crucible. The thermal expansion of quartz is much less than that of the tooling so that the tooling will compress the crucible and even crack it. This compression is minimized by using water cooled tooling kept at a constant water temperature during the process. This will reduce expansion and contraction of the tooling so that the crucible will be easy to remove.
The expansion, contraction and oxidation of the tooling could also be reduced by designing the tooling with a larger inside diameter to leave more quartz starting material to be left over between the crucible and the tooling. The thicker amount of sand will insulate the tooling from the heat so that it will not oxidize as rapidly or expand and contract as much to facilitate in crucible removal. This process, however, is costly because significantly more of the expensive starting material is used. The cost of the high purity starting material is so high that it is impractical to waste it by using any excess during the process. The starting material left over after fusion is not suitable for reuse in the semiconductor grade crucible process since it will contain impurities from the tooling. Therefore it is wise to use only a minimal amount of insulative sand for a barrier to react with the tooling and for heat insulation.
Finely ground quartz material 4 can be obtained through a variety of means, but preferably in a mill using quartz glass pieces as the media. The mill container should also be made of a cylindrical polypropylene material or a cylindrical quartz tube with quartz end plates. The quartz glass media used to grind the material were approximately 6 cm square and 7.5 mm thick. Either crystalline quartz sand or amorphous quartz glass can be ground into fine material.

Claims (3)

We claim:
1. The method of making a quartz glass crucible of low bubble content comprising the steps of preparing a mold having holes therethrough through which a vacuum can be drawn, disposing the mold on a rotatable spindle through which a vacuum can be drawn, rotating the mold while drawing a vacuum on the interior of the mold through said holes, pouring granular quartz material into the mold to form a first layer thereof on the interior of the mold, pouring quartz material finer than said granular quartz material into the mold to form a second layer thereof on the first layer, applying heat to the interior of the mold to melt and fuse the quartz material to form a crucible, and removing the crucible from the mold.
2. The method of claim 1 wherein the granular quartz material has a particle size distribution of about 297 to 105 microns.
3. The method of claim 2 wherein the finer quartz material has a particle size distribution of about 120 to 44 microns.
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Cited By (44)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4838919A (en) * 1987-12-28 1989-06-13 Ppg Industries, Inc. Pretreatment of fused cast refractories
JPH01197382A (en) * 1988-02-03 1989-08-09 Mitsubishi Metal Corp Quartz crucible for pulling-up silicon single crystal
JPH01197381A (en) * 1988-02-03 1989-08-09 Mitsubishi Metal Corp Quartz crucible for pulling-up silicon single crystal
US4935046A (en) * 1987-12-03 1990-06-19 Shin-Etsu Handotai Company, Limited Manufacture of a quartz glass vessel for the growth of single crystal semiconductor
US4946542A (en) * 1988-12-05 1990-08-07 At&T Bell Laboratories Crystal growth method in crucible with step portion
US4949095A (en) * 1988-11-29 1990-08-14 Gte Laboratories Incorporated Fused silica radome
US4956134A (en) * 1987-06-03 1990-09-11 Quartz Et Silice Method of and apparatus for controlling the filling of a mold with a pulverulent refractory material
US4964902A (en) * 1989-02-10 1990-10-23 Quartz & Silice Method of extracting spin cast fused silica
US5015279A (en) * 1989-02-10 1991-05-14 Quartz & Silice Apparatus for extracting spin cast fused silica objects
JPH03208880A (en) * 1990-01-10 1991-09-12 Mitsubishi Materials Corp Quartz crucible and production thereof
US5174801A (en) * 1990-06-25 1992-12-29 Shin-Etsu Quartz Products Co. Ltd. Manufacture of quartz glass crucible for use in the manufacture of single crystal silicon
US5306473A (en) * 1992-01-31 1994-04-26 Toshiba Ceramics Co., Ltd. Quartz glass crucible for pulling a single crystal
US5306388A (en) * 1989-07-28 1994-04-26 Toshiba Ceramics Co., Ltd. Quartz glass crucible for pulling a semiconductor single crystal
US5409891A (en) * 1991-02-22 1995-04-25 Asea Brown Boveri Ltd. Method for producing a rotationally symmetrical molded part of a high-temperature superconductor
FR2726820A1 (en) * 1994-11-15 1996-05-15 Gen Electric QUARTZ CRUCIBLE HAVING A REDUCED BUBBLE CONTENT, METHOD OF MANUFACTURING AND METHOD OF USING THE CRUCIBLE
US5762672A (en) * 1994-07-19 1998-06-09 Shin-Etsu Quartz Products, Ltd. Method for producing a quartz glass crucible
US5895527A (en) * 1996-02-06 1999-04-20 Mitsubishi Materials Silicon Corporation Single crystal pulling apparatus
US5968259A (en) * 1997-08-27 1999-10-19 Shin-Etsu Quartz Products Co., Ltd. High-purity quartz glass and method for the preparation thereof
US6042905A (en) * 1995-02-08 2000-03-28 Futuristic Tile L.L.C. Decorative construction material and methods of its production
EP1020546A4 (en) * 1998-05-25 2001-10-10 Shinetsu Quartz Prod QUARTZ GLASS CRUCIBLE FOR GROWING A SILICON SINGLE CRYSTAL AND METHOD FOR PRODUCING THE SAME
WO2001092169A1 (en) * 2000-05-31 2001-12-06 Heraeus Quarzglas Gmbh & Co. Kg Method for producing quartz glass crucible
US6447601B1 (en) 2001-03-19 2002-09-10 Memc Electronic Materials, Inc. Crystal puller and method for growing monocrystalline silicon ingots
US6510707B2 (en) * 2001-03-15 2003-01-28 Heraeus Shin-Etsu America, Inc. Methods for making silica crucibles
US20030024467A1 (en) * 2001-08-02 2003-02-06 Memc Electronic Materials, Inc. Method of eliminating near-surface bubbles in quartz crucibles
US6546754B1 (en) * 2000-10-27 2003-04-15 General Electric Company Apparatus for silica crucible manufacture
US6672107B2 (en) * 1999-12-22 2004-01-06 Heraeus Quarzglas Gmbh & Co. Kg Quartz glass crucible and process for the production thereof
US20050120945A1 (en) * 2003-12-03 2005-06-09 General Electric Company Quartz crucibles having reduced bubble content and method of making thereof
US20070051297A1 (en) * 2005-09-08 2007-03-08 Heraeus Shin-Etsu America, Inc. Silica glass crucible with barium-doped inner wall
US20070051296A1 (en) * 2005-09-08 2007-03-08 Katsuhiko Kemmochi Silica glass crucible with bubble-free and reduced bubble growth wall
US20070084246A1 (en) * 2005-10-14 2007-04-19 Ohara Inc. Glass forming apparatus and method
DE102008030310B3 (en) * 2008-06-30 2009-06-18 Heraeus Quarzglas Gmbh & Co. Kg Process to fabricate quartz glass crucible with coarse silicon dioxide grains under barrier layer of fine grains
US20090238920A1 (en) * 2008-03-21 2009-09-24 Lewis Ted C Process for making high grade protein product
US20110023773A1 (en) * 2008-03-31 2011-02-03 Japan Super Quartz Corporation Vitreous silica crucible and method of manufacturing the same
US20120141704A1 (en) * 2010-12-01 2012-06-07 Japan Super Quartz Corporation Method of manufacturing vitreous silica crucible, vitreous silica crucible
US20130025319A1 (en) * 2011-07-25 2013-01-31 Heraeus Shin-Etsu America, Inc. Metal and graphite mold and method of making a crucible
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US8524319B2 (en) * 2011-11-18 2013-09-03 Memc Electronic Materials, Inc. Methods for producing crucibles with a reduced amount of bubbles
TWI448592B (en) * 2009-09-07 2014-08-11 Japan Super Quartz Corp Method for manufacturing silica glass crucible
US8857214B2 (en) * 2011-11-18 2014-10-14 Sunedison Semiconductor Limited Methods for producing crucibles with a reduced amount of bubbles
US10066314B2 (en) 2015-07-23 2018-09-04 Globalwafers Co., Ltd. Crystal growing systems and methods including a transparent crucible
WO2021203723A1 (en) * 2020-04-09 2021-10-14 隆基绿能科技股份有限公司 Composite quartz crucible preparation method and composite quartz crucible
CN114481299A (en) * 2022-02-17 2022-05-13 内蒙古鑫晶新材料有限公司 Quartz crucible and manufacturing method thereof
WO2024016879A1 (en) * 2022-07-20 2024-01-25 隆基绿能科技股份有限公司 Crucible melting machine and crucible melting method
CN118307182A (en) * 2024-06-11 2024-07-09 浙江美晶新材料股份有限公司 Semiconductor grade synthetic quartz crucible, preparation method thereof and semiconductor grade monocrystalline silicon growth method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3853520A (en) * 1972-12-27 1974-12-10 K Rau Method for making hollow cylinders of vitreous silica by vacuum heating
US3902885A (en) * 1972-12-27 1975-09-02 Heraeus Schott Quarzschmelze Apparatus for making hollow cylinders of vitreous silica
JPS5272714A (en) * 1975-12-15 1977-06-17 Ouchi Nobutoshi Method of production of glass for decoration form waste glass
US4416680A (en) * 1980-04-15 1983-11-22 Heraeus Quarzschmelze Gmbh Method of making quartz glass crucibles, and apparatus carrying out the method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3853520A (en) * 1972-12-27 1974-12-10 K Rau Method for making hollow cylinders of vitreous silica by vacuum heating
US3902885A (en) * 1972-12-27 1975-09-02 Heraeus Schott Quarzschmelze Apparatus for making hollow cylinders of vitreous silica
JPS5272714A (en) * 1975-12-15 1977-06-17 Ouchi Nobutoshi Method of production of glass for decoration form waste glass
US4416680A (en) * 1980-04-15 1983-11-22 Heraeus Quarzschmelze Gmbh Method of making quartz glass crucibles, and apparatus carrying out the method

Cited By (65)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4956134A (en) * 1987-06-03 1990-09-11 Quartz Et Silice Method of and apparatus for controlling the filling of a mold with a pulverulent refractory material
US4956208A (en) * 1987-12-03 1990-09-11 Shin-Etsu Handotai Co., Ltd. Manufacture of a quartz glass vessel for the growth of single crystal semiconductor
US4935046A (en) * 1987-12-03 1990-06-19 Shin-Etsu Handotai Company, Limited Manufacture of a quartz glass vessel for the growth of single crystal semiconductor
EP0319031A3 (en) * 1987-12-03 1990-08-01 Shin-Etsu Handotai Company, Limited Manufacture of a quartz glass vessel for the growth of single crystal semiconductor
DE3842680A1 (en) * 1987-12-28 1989-07-06 Ppg Industries Inc TREATMENT OF MELTED, MOLDED, FIREPROOF MATERIAL
US4838919A (en) * 1987-12-28 1989-06-13 Ppg Industries, Inc. Pretreatment of fused cast refractories
JPH01197381A (en) * 1988-02-03 1989-08-09 Mitsubishi Metal Corp Quartz crucible for pulling-up silicon single crystal
JPH01197382A (en) * 1988-02-03 1989-08-09 Mitsubishi Metal Corp Quartz crucible for pulling-up silicon single crystal
US4949095A (en) * 1988-11-29 1990-08-14 Gte Laboratories Incorporated Fused silica radome
US4946542A (en) * 1988-12-05 1990-08-07 At&T Bell Laboratories Crystal growth method in crucible with step portion
US4964902A (en) * 1989-02-10 1990-10-23 Quartz & Silice Method of extracting spin cast fused silica
US5015279A (en) * 1989-02-10 1991-05-14 Quartz & Silice Apparatus for extracting spin cast fused silica objects
US5306388A (en) * 1989-07-28 1994-04-26 Toshiba Ceramics Co., Ltd. Quartz glass crucible for pulling a semiconductor single crystal
JPH03208880A (en) * 1990-01-10 1991-09-12 Mitsubishi Materials Corp Quartz crucible and production thereof
US5174801A (en) * 1990-06-25 1992-12-29 Shin-Etsu Quartz Products Co. Ltd. Manufacture of quartz glass crucible for use in the manufacture of single crystal silicon
US5409891A (en) * 1991-02-22 1995-04-25 Asea Brown Boveri Ltd. Method for producing a rotationally symmetrical molded part of a high-temperature superconductor
US5306473A (en) * 1992-01-31 1994-04-26 Toshiba Ceramics Co., Ltd. Quartz glass crucible for pulling a single crystal
US5762672A (en) * 1994-07-19 1998-06-09 Shin-Etsu Quartz Products, Ltd. Method for producing a quartz glass crucible
FR2726820A1 (en) * 1994-11-15 1996-05-15 Gen Electric QUARTZ CRUCIBLE HAVING A REDUCED BUBBLE CONTENT, METHOD OF MANUFACTURING AND METHOD OF USING THE CRUCIBLE
US6042905A (en) * 1995-02-08 2000-03-28 Futuristic Tile L.L.C. Decorative construction material and methods of its production
US5895527A (en) * 1996-02-06 1999-04-20 Mitsubishi Materials Silicon Corporation Single crystal pulling apparatus
US5968259A (en) * 1997-08-27 1999-10-19 Shin-Etsu Quartz Products Co., Ltd. High-purity quartz glass and method for the preparation thereof
EP1020546A4 (en) * 1998-05-25 2001-10-10 Shinetsu Quartz Prod QUARTZ GLASS CRUCIBLE FOR GROWING A SILICON SINGLE CRYSTAL AND METHOD FOR PRODUCING THE SAME
US6797061B2 (en) 1998-05-25 2004-09-28 Shin Etsu Quartz Products Co., Ltd. Quartz glass crucible for pulling up silicon single crystal and production method therefor
US6672107B2 (en) * 1999-12-22 2004-01-06 Heraeus Quarzglas Gmbh & Co. Kg Quartz glass crucible and process for the production thereof
US20030074920A1 (en) * 2000-05-31 2003-04-24 Yasuo Ohama Method for producing quartz glass crucible
WO2001092169A1 (en) * 2000-05-31 2001-12-06 Heraeus Quarzglas Gmbh & Co. Kg Method for producing quartz glass crucible
US6886364B2 (en) 2000-05-31 2005-05-03 Heraeus Quarzglas Gmbh & Co. Kg Method for producing quartz glass crucible
US6546754B1 (en) * 2000-10-27 2003-04-15 General Electric Company Apparatus for silica crucible manufacture
US6510707B2 (en) * 2001-03-15 2003-01-28 Heraeus Shin-Etsu America, Inc. Methods for making silica crucibles
US6447601B1 (en) 2001-03-19 2002-09-10 Memc Electronic Materials, Inc. Crystal puller and method for growing monocrystalline silicon ingots
US20030024467A1 (en) * 2001-08-02 2003-02-06 Memc Electronic Materials, Inc. Method of eliminating near-surface bubbles in quartz crucibles
US20050120945A1 (en) * 2003-12-03 2005-06-09 General Electric Company Quartz crucibles having reduced bubble content and method of making thereof
US20070051296A1 (en) * 2005-09-08 2007-03-08 Katsuhiko Kemmochi Silica glass crucible with bubble-free and reduced bubble growth wall
US7383696B2 (en) 2005-09-08 2008-06-10 Heraeus Shin-Etsu America, Inc. Silica glass crucible with bubble-free and reduced bubble growth wall
US7427327B2 (en) 2005-09-08 2008-09-23 Heraeus Shin-Etsu America, Inc. Silica glass crucible with barium-doped inner wall
US20070051297A1 (en) * 2005-09-08 2007-03-08 Heraeus Shin-Etsu America, Inc. Silica glass crucible with barium-doped inner wall
US8087264B2 (en) * 2005-10-14 2012-01-03 Ohara Inc. Glass forming apparatus and method
US20070084246A1 (en) * 2005-10-14 2007-04-19 Ohara Inc. Glass forming apparatus and method
US20090238920A1 (en) * 2008-03-21 2009-09-24 Lewis Ted C Process for making high grade protein product
CN104947189A (en) * 2008-03-31 2015-09-30 日本超精石英株式会社 Quartz glass crucible and process for producing the same
US20110023773A1 (en) * 2008-03-31 2011-02-03 Japan Super Quartz Corporation Vitreous silica crucible and method of manufacturing the same
CN101983262A (en) * 2008-03-31 2011-03-02 日本超精石英株式会社 Quartz glass crucible and manufacturing method thereof
EP2264226A4 (en) * 2008-03-31 2011-07-27 Japan Super Quartz Corp Quartz glass crucible and process for producing the same
TWI385132B (en) * 2008-05-28 2013-02-11 Japan Super Quartz Corp Silica glass crucible and method for manufacturing the same
JP2010013339A (en) * 2008-06-30 2010-01-21 Shinetsu Quartz Prod Co Ltd Manufacturing process of quartz glass crucible
US8347650B2 (en) 2008-06-30 2013-01-08 Heraeus Quarzglas Gmbh & Co. Kg Method of producing a quartz glass crucible
EP2141131A2 (en) 2008-06-30 2010-01-06 Heraeus Quarzglas GmbH & Co. KG Method of producing a quartz glass crucible
TWI395719B (en) * 2008-06-30 2013-05-11 Shinetsu Quartz Prod Method of producing a quartz glass crucible
EP2141131A3 (en) * 2008-06-30 2013-12-25 Heraeus Quarzglas GmbH & Co. KG Method of producing a quartz glass crucible
DE102008030310B3 (en) * 2008-06-30 2009-06-18 Heraeus Quarzglas Gmbh & Co. Kg Process to fabricate quartz glass crucible with coarse silicon dioxide grains under barrier layer of fine grains
TWI448592B (en) * 2009-09-07 2014-08-11 Japan Super Quartz Corp Method for manufacturing silica glass crucible
US9469560B2 (en) * 2010-12-01 2016-10-18 Japan Super Quartz Corporation Method of manufacturing vitreous silica crucible, vitreous silica crucible
US20120141704A1 (en) * 2010-12-01 2012-06-07 Japan Super Quartz Corporation Method of manufacturing vitreous silica crucible, vitreous silica crucible
US9216923B2 (en) * 2011-07-25 2015-12-22 Shin-Etsu Quartz Products Co., Ltd. Metal and graphite mold and method of making a crucible
US20130025319A1 (en) * 2011-07-25 2013-01-31 Heraeus Shin-Etsu America, Inc. Metal and graphite mold and method of making a crucible
US8857214B2 (en) * 2011-11-18 2014-10-14 Sunedison Semiconductor Limited Methods for producing crucibles with a reduced amount of bubbles
US8524319B2 (en) * 2011-11-18 2013-09-03 Memc Electronic Materials, Inc. Methods for producing crucibles with a reduced amount of bubbles
US10066314B2 (en) 2015-07-23 2018-09-04 Globalwafers Co., Ltd. Crystal growing systems and methods including a transparent crucible
US10557213B2 (en) 2015-07-23 2020-02-11 Globalwafers Co., Ltd. Crystal growing systems and methods including a transparent crucible
WO2021203723A1 (en) * 2020-04-09 2021-10-14 隆基绿能科技股份有限公司 Composite quartz crucible preparation method and composite quartz crucible
CN113510824A (en) * 2020-04-09 2021-10-19 隆基绿能科技股份有限公司 Preparation method of composite quartz crucible and composite quartz crucible
CN114481299A (en) * 2022-02-17 2022-05-13 内蒙古鑫晶新材料有限公司 Quartz crucible and manufacturing method thereof
WO2024016879A1 (en) * 2022-07-20 2024-01-25 隆基绿能科技股份有限公司 Crucible melting machine and crucible melting method
CN118307182A (en) * 2024-06-11 2024-07-09 浙江美晶新材料股份有限公司 Semiconductor grade synthetic quartz crucible, preparation method thereof and semiconductor grade monocrystalline silicon growth method

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